A kind of synthetic method of 2-amino-4-acetamidoanisole

A technology of acetamidoanisole and p-aminoanisole, which is applied in the field of synthesis of 2-amino-4-acetamidoanisole, can solve problems such as increased raw material costs, achieve low equipment corrosion, and avoid raw materials being easy to use. Oxidation, high conversion effect

Active Publication Date: 2020-04-07
NINGXIA ZHONGSHENG NEW TECH CO LTD
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Problems solved by technology

[0004] The second preparation method is to use 2-nitro-4-acetamidoanisole as a raw material to obtain 3-amino-4-alkoxyacetanilide through one-step catalytic hydrogenation. Although this method has a short route, the productive rate of the product is , high purity, but the cost of raw materials is greatly increased

Method used

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  • A kind of synthetic method of 2-amino-4-acetamidoanisole
  • A kind of synthetic method of 2-amino-4-acetamidoanisole
  • A kind of synthetic method of 2-amino-4-acetamidoanisole

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Embodiment 1

[0062] Embodiment 1, synthetic 2-amino-4-acetamidoanisole

[0063] (1) etherification reaction

[0064] Add 1570kg of p-nitrochlorobenzene and 1920kg of methanol to a 3000L etherification reaction kettle, then raise the reaction temperature to 70°C, gradually add 420kg of sodium hydroxide to it, and carry out the etherification reaction. Heat filtration at 40°C to obtain p-nitroanisole. The yield is 97.2%, and the melting point is 50.5-52.0°C. According to GC analysis, its purity is 99.7%, and the filtrate enters the methanol separation tower, and the methanol is recovered through distillation.

[0065] (2) One catalytic hydrogenation reduction reaction

[0066] With 6000kg p-nitroanisole, 120kg catalyst Ni-Mo-Co-Li (wherein the weight percent of Ni, Mo, Co, Li is 90.0%, 5.0%, 2.0% and 3%, carrier is modified alumina) Add 7500L methanol in the 16000L reactor, feed nitrogen into the reactor, evacuate the air, repeat 5 times, to completely remove the air in the reactor, then...

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Abstract

The invention discloses a synthesis method of 2-amino-4-acetamino anisole. The synthesis method comprises the following steps: (1) carrying out a primary catalytic hydrogenation reduction reaction onp-nitroanisole and hydrogen in the presence of a catalyst A to obtain p-methoxyaniline; (2) carrying out an acetylation reaction on the p-methoxyaniline to obtain p-acetanisidine; (3) carrying out a nitration reaction on the p-acetanisidine to obtain 2-nitro-4-acetamino anisole; and (4) carrying out a secondary catalytic hydrogenation reduction reaction on the 2-nitro-4-acetamino anisole and hydrogen in the presence of a catalyst B to obtain 2-amino-4-acetamino anisole. 2-amino-4-acetamino anisole is synthesized by using a method sequentially comprising acylation, nitration and reduction, so that the problems that raw materials are easily oxidized, the amount of side reactions is large and a product is difficult to separate and low in purity in a traditional directional acylation process are avoided; and the purity of the product synthesized by using the method disclosed by the invention can reach 99.5%-99.8%.

Description

technical field [0001] The invention relates to a synthesis method of 2-amino-4-acetamidoanisole, which belongs to the field of organic chemical synthesis. Background technique [0002] 2-Amino-4-acetamidoanisole is an important intermediate for the preparation of C.I. Disperse Blue 79 and Disperse Violet 58 and other series of disperse dyes, especially the coupling component for the preparation of disperse dark blue H-GL with a large output. It is sold in domestic and foreign markets The demand is huge. The method of producing 2-amino-4-acetamidoanisole at home and abroad mainly contains following two kinds at present. [0003] The first preparation method is to use 2,4-dinitrochlorobenzene (or its intermediate product) as raw material to obtain 2-amino-4-acetamidoanisole through etherification, reduction and selective acylation. In this process route, iron powder, alkali sulfide or hydrazine hydrate was usually used in the reduction step before, which caused serious envi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/02C07C233/43B01J23/887
CPCB01J23/8872C07C201/12C07C213/02C07C231/02C07C205/37C07C217/84C07C233/25C07C233/43
Inventor 王明和郝新敏王春敏
Owner NINGXIA ZHONGSHENG NEW TECH CO LTD
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